Patent GB-1029165-A (GB)
Title: Method and apparatus for measuring cloud point temperatures
Inventor: CRESPIN GEORGE THEODORE FLORIM
IPC: G01N25/04
Filed: 1964-07-28
Abstract: 1,029,165. Automatic control. SHELL INTERNATIONAL RESEARCH MAATSCHAPPY N.V. July 28, 1964,No. 30018/64. Heading G3R. [Also in Division G1] In determination of cloudpoint temperature for oils and the like or a temperature correlated with the cloud point, a sample of the oil is cooled progressively from a temperature in excess of that to be determined in such manner that convection flow occurs at the initiation of the cooling, and ceases at the cloudpoint temperature due to the formation of wax crystals in the oil; the cessation of convection flow being determined by measurement of the temperature difference at vertically displaced positions of the oil, which assumes a fixed value, e.g. zero, at cloudpoint temperature, which is determined by measurement of the oil temperature at an intervening point. In Fig. 1 a sample vessel 1 of glass or plastic containing oil under test is surrounded by a metal block 2 provided on opposite sides with thermoelectric cooling modules 3 and having a watercooled heat sink 4 protected by a thermostat (not shown) operative on cooling water failure to interrupt the D.C. energization of the modules from mains energized power unit 6 over reversing switch 8. A thermocouple 9 at mid height of vessel 1 and an indicating instrument 10 measures the sample temperature, and thermistors 11,12 are placed axially of the sample at points below the cooling modules and midway between couple 9 and the top of the modules. The thermistors are connected in opposed arms of a differential temperature measuring bridge 13, whose output is connected through bias EMF 14 and a time delay device 15 to a transistorised Schmitt relay 16 operative on a small D.C. input rise and remaining operated until the input falls below a critical input value A stabilized mains energised power supply 17 energizes the bridge, the bias supply, and the relay; the latter being arranged to clamp the indicating instrument on cloudpoint being reached and to position the reverse switch 8. In operation, a press switch 18 excites power supply 6 to energize the thermoelectric modules to cool the sample and also to disable the time delay device 15. Convection currents are set up in the sample (Fig. 2 not shown) and thermistor 12 becomes warmer than thermistor 11 so that the bridge output develops a certain amplitude and polarity. At cloudpoint, convection ceases and thermistor 12 becomes cooled by conduction into the surrounding metal block, so that the bridge output falls in amplitude and reverses in polarity. The Schmitt trigger operates to clamp the indicator 10 indicating the temperature of thermocouple 9 at cloudpoint and to reverse the current to the thermoelectric modules so as to heat the sample, and thus to zeroise the temperature difference between thermistors 11,12 so that the trigger reverts and switches off at 6 the current to the thermoelectric modules. Further triggering of 16 at initiation of the following test is prevented by time delay device 15, which is opened on operation of press switch 18 to disconnect the trigger for a predetermined time during which a temperature difference develops between thermisters 11,12. In a modification (Fig. 3 not shown) for continuous measurement and recording of cloud point of a process stream, a sample from a fast loop is bled through a solenoid valve controlled by a command device operated by the schmitt trigger to flush the sample vessel for a fixed period and to leave a sample in the vessel. The command device then operates a reversing switch to initiate cooling of the sample by the combination of metal block, thermoelectric modules,and heat sink shown as, and at cloud point the trigger operates the command device to flush the sample vessel, the reverse switch to heat the sample, and initiated time delay device to remove the input to the trigger, after which the cycle is repeated. The sample temperatures are recorded as a sawtooth from which the successive cloud point temperatures may be deduced. A peak sensitive device (not shown) develops signals corresponding to last recorded temperature peaks which are used to control a process to maintain a constant cloud point or prevent this from exceeding a fixed limit. Resistance thermometers or thermocouples are stated to be replaceable for thermistors.